CN106018294B - A method of detection nano-titanium dioxide down flop property - Google Patents
A method of detection nano-titanium dioxide down flop property Download PDFInfo
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- CN106018294B CN106018294B CN201610455247.1A CN201610455247A CN106018294B CN 106018294 B CN106018294 B CN 106018294B CN 201610455247 A CN201610455247 A CN 201610455247A CN 106018294 B CN106018294 B CN 106018294B
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Abstract
The invention belongs to nano ZnO detection fields, and in particular to a kind of detection method of nano-titanium dioxide down flop property.A method of detection nano-titanium dioxide down flop property, comprising the following steps: a, solvent preparation: according to mass ratio, by alkyd resin: ethyl acetate=0.5~1.5:0.5~1.5 mixing obtains solvent；B, prepared by test fluid: by nano-titanium dioxide to be measured, solvent and bead according to 2~3:35 of weight ratio~45:5~15, concussion 45~120min of mixing obtains test fluid；C, it detects: being taken in test droplets to black and white paper with dropper, scraping blade, it is dry, it obtains with a thickness of 25~100 μm of films, detects 15 °, 25 °, 45 °, 75 ° and 110 ° of film of L, a, b value respectively；D, with the L of standard specimen0、a0、b0Value is compared, and utilizes formula I, calculates the Δ E value of nano-titanium dioxide and standard specimen to be measured.The method of the present invention is simple, can fast and accurately detect the down flop property of different nano-titanium dioxides.
Description
Technical field
The invention belongs to nano ZnO detection fields, and in particular to a kind of nano-titanium dioxide down flop property
Detection method.
Background technique
Pigment changeable colors along with angle, i.e., under visible light illumination, when light source position is constant, with the change of viewing angle, pigment
Color and gloss also changed pigment therewith, this phenomenon be occur in the multilayered structure of pigment due to visible light it is anti-
It penetrates, interfere and absorbs and generate, so pigment changeable colors along with angle is also referred to as interference of light pigment.Interference of light pigment is international in recent years
Upper ornament materials, cosmetics and the new research hotspot of anti-counterfeit field.
Wherein, gold redrock nano-titanium dioxide is because having excellent ultraviolet shielded ability and down flop property to be answered extensively
For in automobile coating industry.
Application No. is " 200410053451.8 ", a kind of entitled " rutile type nano of high stable, high transparency
Titanium deoxide slurry and its dispersion preparation method ", disclose it is a kind of by dispersion resin, rutile type nano titanic oxide powder, point
The rutile type nano titanic oxide slurry of powder and solvent composition, is prepared into after pre-dispersed, high speed dispersion and ultrasonic disperse
It arrives.
It is entitled " Production of cobalt-titanium series random chromo pigment " application No. is " 200510105419.4 ", it is public
It has opened a kind of, as host material, to be deposited with wet chemistry method on mica titanium surface certain thickness by pretreated mica titanium
Cobalt hydroxide, calcining obtain the yellow-green pigment changeable colors along with angle for waiting multiple colors interconversion of soil.
Application No. is " 201410018802.5 ", entitled " decorative and weatherability and excellent changeable colors along with angle type vehicle
With metallic finishe ", disclose it is a kind of by it is colorless and transparent and with sufficiently wear-resistant property and hardness Lacquer finish finishing coat, it is transparent it is coloured, include
There is the floating coating of plain color pigments and fillers and changeable colors along with angle type pigments and fillers component and there is enough tinting strength, tinting powers and covering power, include plain color face
The opaque primary coat paint of filler, which combines, to be constituted, and floating coating and primary coat paint are divided on the basis of scheduled universal basic paste formula
Floating coating paste formula and the primary coat of the corresponding color component being made of accordingly plain color or changeable colors along with angle type pigments and fillers are not added
The semi-finished product mill base spraying that paint paste formula is formulated is constituted.
In conclusion being related to the preparation method of pigment changeable colors along with angle mostly in the prior art, it is not directed to specific detection method.
And the changeable colors along with angle for detecting nano-titanium dioxide at present is all that corresponding automobile is made according to using formula in nano-titanium dioxide
After paint detect application product transparency or light transmittance, result in this way nano-titanium dioxide be difficult to judge it before application be
No qualification, therefore the method for establishing a kind of changeable colors along with angle of quick, easy direct detection nano-titanium dioxide is very necessary.
Summary of the invention
Technical problem to be solved by the invention is to provide it is a kind of quickly, accurate, simple detection nano-titanium dioxide with
The method of the heterochromatic performance in angle.
A kind of method for detecting nano-titanium dioxide down flop property of the present invention, comprising the following steps:
A, prepared by solvent: according to mass ratio, by alkyd resin: ethyl acetate=0.5~1.5:0.5~1.5 mixing obtains
Solvent；
B, test fluid prepare: by nano-titanium dioxide to be measured, solvent and bead according to 2~3:35 of weight ratio~45:5~
15, concussion 45~120min of mixing obtain test fluid；
C, it detects: being taken in test droplets to black and white paper with dropper, scraping blade, it is dry, it obtains with a thickness of 25~100 μm of films,
15 °, 25 °, 45 °, 75 ° and 110 ° of film of L, a, b value is detected respectively；
D, it calculates: by measurement to L, a, b value of test sample nano-titanium dioxide and the L of standard specimen0、a0、b0Value is compared,
And formula I is utilized, calculate the Δ E value of nano-titanium dioxide and standard specimen to be measured；
(Ⅰ)
Δ L=L-L under equal angular, in formula0, Δ a=a-a0, Δ b=b-b0。
Further, technical solution more preferably, a kind of detection nano-titanium dioxide color travel described above
The method of energy, wherein according to mass ratio, alkyd resin: ethyl acetate=1:1 in a step.
Further, technical solution more preferably, a kind of detection nano-titanium dioxide color travel described above
Can method, wherein in b step nano-titanium dioxide to be measured, solvent A and bead weight ratio 2.67:40:10.
A kind of method detecting nano-titanium dioxide down flop property described above, is wherein shaken in b step using quick worker
Swing device concussion.
Further, technical solution more preferably, a kind of detection nano-titanium dioxide color travel described above
The method of energy, wherein concussion mixes 45~60min in b step.
A kind of method detecting nano-titanium dioxide down flop property described above, wherein drying temperature is in step c
40~60 DEG C.
A kind of method detecting nano-titanium dioxide down flop property described above, wherein detects in step c and uses
Five angle color difference meter of MA68.
A kind of method detecting nano-titanium dioxide down flop property described above, is wherein applied in step c using silk stick
Cloth device scraping blade.
The present invention relates to a kind of methods for detecting nano-titanium dioxide down flop property, and method is simple, can be quick, quasi-
The down flop property of the true different nano-titanium dioxides of detection, to be conducive to the production control of nano-titanium dioxide manufacturing enterprise
System, while being conducive to that nano-titanium dioxide user is instructed to select suitable nanometer titanium dioxide titanium products according to their own needs.
Specific embodiment
A kind of method for detecting nano-titanium dioxide down flop property of the present invention, comprising the following steps:
A, prepared by solvent: according to mass ratio, by alkyd resin: ethyl acetate=0.5~1.5:0.5~1.5 mixing obtains
Solvent；
B, test fluid prepare: by nano-titanium dioxide to be measured, solvent and bead according to 2~3:35 of weight ratio~45:5~
15, it is fitted into the glass container that can be sealed, concussion 45~120min of mixing obtains test fluid；
C, it detects: being taken in test droplets to black and white paper with dropper, scraping blade, it is dry, it obtains with a thickness of 25~100 μm of films,
15 °, 25 °, 45 °, 75 ° and 110 ° of film of L, a, b value is detected respectively；
D, it calculates: by measurement to L, a, b value of test sample nano-titanium dioxide and the L of standard specimen0、a0、b0Value is compared,
And formula I is utilized, calculate the Δ E value of nano-titanium dioxide and standard specimen to be measured；
(Ⅰ)
Δ L=L-L under equal angular, in formula0, Δ a=a-a0, Δ b=b-b0。
Further, technical solution more preferably, a kind of detection nano-titanium dioxide color travel described above
The method of energy, wherein according to mass ratio, alkyd resin: ethyl acetate=1:1 in a step.In addition to alkyd resin and ethyl acetate,
The resin that can also select other transparencys and the esters solvent that can be dissolved are mixed as flux.
Further, technical solution more preferably, a kind of detection nano-titanium dioxide color travel described above
Can method, wherein in b step nano-titanium dioxide to be measured, solvent A and bead weight ratio 2.67:40:10.Wherein, glass
The addition of glass pearl is as abrasive media material, and the abrasive medias such as other zirconium pearls with said function can replace bead.
A kind of method detecting nano-titanium dioxide down flop property described above, is wherein shaken in b step using quick worker
Swing device concussion.
Further, technical solution more preferably, a kind of detection nano-titanium dioxide color travel described above
The method of energy, wherein preferably concussion mixes 45~60min in b step.Wherein, the purpose of concussion is by nano material and other materials
While material is uniformly mixed, can also break up the particulate abrasive of reunion keeps nano material fully dispersed in a solvent, experiments have shown that
Grinding 45min or more can reach preferable grinding effect.
A kind of method detecting nano-titanium dioxide down flop property described above, wherein drying temperature is in step c
40~60 DEG C.
A kind of method detecting nano-titanium dioxide down flop property described above, wherein detects in step c and uses
Five angle color difference meter of MA68 can compare after detecting 15 °, 25 °, 45 °, 75 ° and 110 ° of film of L, a, b value respectively with standard specimen,
Sample and standard specimen sense organ difference, then the brightness difference by comparing L value difference value energy response sample are directly observed by the naked eye,
And same bigger its down flop property of reaction of sample different angle a, b difference is more obvious.
A kind of method detecting nano-titanium dioxide down flop property described above, is wherein applied in step c using silk stick
Cloth device scraping blade.Present invention selection carries out scraping blade on black and white paper, is because energy is intuitive on black and white plate and after scraping blade processing simultaneously
Observe the transparency of sample.
In addition, color effects caused by vision depend on the light of body surface reflection to three kinds of pyramidal cells in human eye
The stimulation degree of generation.Stimulation respective function is respectively R (λ), G caused by light of three kinds of pyramidal cells to different wave length λ
(λ), B (λ).When the body surface reflectance spectrum that human eye receives is S (λ), color which cashes out for (R, G,
B)
When adjusting the spectrum of surface reflection, the color that object shows will change.
In same object surface, since technique limits, the thickness of film layer itself has certain inhomogeneities.From difference
The spectrum S (λ) reflected at position can change with the thicknesses of layers that the position goes out and be changed, so that apparent color
Variation is generated, is cashed as color difference.
For general color showing method in accordance with CIELAB system, it is a uniform color space, every kind of face in the world
Color table is shown as (L, a, b), and wherein the intensity of light is shown in L, and a indicates red green degree, and b indicates yellow blue degree.(L, a,
B) it can be obtained by (R, G, B) value by linear transformation.To be consistent with general international standard, color measuring used hereinafter
CIELAB method is used with color difference characterization.
The size of color difference is generally judged with Δ E, Δ E represents color difference comprehensive deviation amount, and numerical value is equal to the quadratic sum of L, a, b
Evolution again.
Δ E=[(Δ L)2+(Δa)2+(Δb)2]1/2
Δ L=LSample-LStandard(lightness difference)
Δ a=aSample-aStandard(red green difference)
Δ b=bSample-bStandard(yellow blue difference)
+ Δ L indicates partially white, and-Δ L indicates partially black；
+ Δ a indicates partially red, and-Δ a indicates partially green；
+ Δ b indicates partially yellow, and-Δ b indicates partially blue；
The size of 1 Δ E total color difference of table
Δ E is smaller, and to represent color difference smaller.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
One, the down flop property of nano-titanium dioxide standard specimen (certain external product) is detected
(1) alkyd resin and ethyl acetate are mixed into solvent according to mass ratio 1:1；
(2) 2.67g nano-titanium dioxide standard specimen to be measured and 40g solvent are weighed respectively in glass, add 10g glass
Then pearl covers tightly bottle cap；The main component of the nano-titanium dioxide standard specimen to be measured is titanium dioxide and surface treated oxidation
Zirconium and aluminium oxide, specific surface area are about 45m2/g；
(3) symmetrical vial sample is shaken into 45min mounted in fast on hand；
(4) it is dripped on black and white paper with dropper sampling, with 25 μm of silk stick scraping blades, uses five angle color difference meter of MA68 after 50 DEG C of drying
15 °, 25 °, 45 °, 45 ° and 110 ° of L, a, b value of film the results are shown in Table 2 on detection blackboard:
5 angle colorations values of 2 standard specimen of table (certain external product)
| 15° | 25° | 45° | 75° | 110° | |
| L | 37.57 | 34.26 | 33.44 | 34.83 | 36.01 |
| a | 1.48 | 0.59 | 0.24 | -0.12 | -0.52 |
| b | -15.29 | -17.61 | -18.45 | -18.56 | -18.08 |
Standard specimen has an apparent changeable colors along with angle effect as seen from Table 2,25 °, 45 °, 75 °, 110 ° of a and b value with 15 °
A and b value between difference be respectively 0.89,1.24,1.60,2.00；2.32,3.16,3.27,2.79.Between different angle
Chromaticity coordinate difference difference show that its different angle color difference is bigger more greatly, changeable colors along with angle effect is more obvious.
Two, the down flop property of nano-titanium dioxide sample 1 to be measured is detected
(1) alkyd resin and ethyl acetate are mixed into solvent according to mass ratio 1:1；
(2) 2.67g nano-titanium dioxide sample 1 to be measured and 40g solvent are weighed respectively in glass, add 10g glass
Then glass pearl covers tightly bottle cap；The main component of the nano-titanium dioxide sample 1 to be measured is titanium dioxide and surface treated
Zirconium oxide and aluminium oxide, specific surface area are about 70m2/g；
(3) symmetrical vial sample is shaken into 60min mounted in fast on hand；
(4) it is dripped on black and white paper with dropper sampling, with 50 μm of silk stick scraping blades, five angle color difference meter of MA68 is used after 60 DEG C of dryings
15 °, 25 °, 45 °, 45 ° and 110 ° of L, a, b value of film the results are shown in Table 3 on detection blackboard:
5 angle colorations values of 3 sample 1 of table
| 15° | 25° | 45° | 75° | 110° | |
| L | 33.42 | 31.16 | 30.15 | 31.35 | 32.54 |
| a | 1.6 | 0.75 | 0.44 | 0.12 | -0.25 |
| b | -14.07 | -15.72 | -16.55 | -16.85 | -16.59 |
As seen from Table 3 standard specimen have apparent changeable colors along with angle effect, compared with standard specimen, 15 ° and 25 °, 45 °, 75 °,
110 ° of L, a and b difference is respectively △ L=4.15, and 3.1,3.29,3.48,3.47；△ a=-0.12, -0.16, -0.2, -
0.28, -0.27；△ b=-1.22, -1.89, -1.9, -1.71, -1.49.It is calculated using formula (I), 15 ° and 25 °,
45 °, 75 °, 110 ° of △ E value be respectively 4.33,3.63,3.8,3.88,3.79, average △ E=3.886, average 2 < △ E
≤ 4, illustrate that there is also certain gap between sample to be tested 1 and standard specimen, i.e. the down flop property of sample to be tested 1 is poorer than standard specimen.
Meanwhile the difference between its 25 ° of sample to be tested 1,45 °, 75 °, 110 ° of a and b value and 15 ° of a and b value is distinguished
It is 0.85,1.16,1.48,1.85；1.65,2.48,2.78,2.52.Compare standard specimen, the color between 1 different angle of sample to be tested
Product coordinate difference is smaller, illustrates that its changeable colors along with angle effect is poorer than standard specimen.
Embodiment 2 detects the down flop property of nano-titanium dioxide sample 2 to be measured
(1) alkyd resin and ethyl acetate are mixed into solvent according to mass ratio 1:1；
(2) 2.67g nano-titanium dioxide sample 2 to be measured and 40g solvent are weighed respectively in glass, add 10g glass
Then glass pearl covers tightly bottle cap；The main component of the nano-titanium dioxide sample 2 to be measured is titanium dioxide and surface treated
Zirconium oxide and aluminium oxide, specific surface area are about 85m2/g；
(3) symmetrical vial sample is shaken into 45min mounted in fast on hand；
(4) it is dripped on black and white paper with dropper sampling, with 25 μm of silk stick scraping blades, uses five angle color difference meter of MA68 after 50 DEG C of drying
15 °, 25 °, 45 °, 45 ° and 110 ° of L, a, b value of film the results are shown in Table 4 on detection blackboard:
5 angle colorations values of 4 sample 2 of table
| 15° | 25° | 45° | 75° | 110° | |
| L | 38.71 | 36.78 | 36.34 | 38.09 | 39.3 |
| a | 1.3 | 0.77 | 0.43 | -0.13 | -0.66 |
| b | -19.29 | -20.89 | -21.56 | -21.43 | -20.59 |
As seen from Table 4 standard specimen 2 have apparent changeable colors along with angle effect, compared with standard specimen, 15 ° and 25 °, 45 °, 75 °,
110 ° of L, a and b difference is respectively △ L=-1.14, and -2.52, -2.9, -3.26, -3.29；△ a=1.18, -0.18, -
0.19,0.01,0.14；△ b=4,3.28,3.11,2.87,2.51.Be calculated using formula (I), 15 ° and 25 °, 45 °,
75 °, 110 ° of △ E value be respectively 4.32,4.14,4.26,4.34,4.14, average △ E=4.24, average 4 < △ E, explanation
There is also very big gap between sample to be tested 2 and standard specimen, i.e. the down flop property of sample to be tested 2 is poorer than standard specimen.
Meanwhile the difference between its 25 ° of sample to be tested 2,45 °, 75 °, 110 ° of a and b value and 15 ° of a and b value is respectively
0.53,0.87,1.43,1.96；1.60,2.27,2.14,1.3.Standard specimen is compared, the chromaticity between 2 different angle of sample to be tested is sat
It is smaller to mark difference, also illustrates that its changeable colors along with angle effect is poorer than standard specimen.
Claims (8)
1. a kind of method for detecting nano-titanium dioxide down flop property, it is characterised in that the following steps are included:
A, prepared by solvent: according to mass ratio, by alkyd resin: ethyl acetate=0.5~1.5:0.5~1.5 mixing obtains molten
Agent；
B, prepared by test fluid: by nano-titanium dioxide to be measured, solvent and bead according to 2~3:35 of weight ratio~45:5~15,
Concussion 45~120min of mixing, obtains test fluid；
C, it detects: being taken in test droplets to black and white paper with dropper, scraping blade, it is dry, it obtains with a thickness of 25~100 μm of films, respectively
L, a, b value of 15 °, 25 °, 45 °, 75 ° and 110 ° of film of detection；
D, it calculates: by measurement to L, a, b value of test sample nano-titanium dioxide and the L of standard specimen0、a0、b0Value is compared, and benefit
With formula I, the Δ E value of nano-titanium dioxide and standard specimen to be measured is calculated；
(Ⅰ)
Δ L=L-L under equal angular, in formula0, Δ a=a-a0, Δ b=b-b0；
E, 15 °, 25 °, 45 °, 75 °, the arithmetic mean of instantaneous value of 110 ° of △ E value are calculated, nanometer to be measured is judged according to the average value of △ E
The down flop property of titanium dioxide and the gap of standard specimen；
When △ E is 0~0.25, indicate that color difference is very small or does not have；
When △ E is 0.25~0.5, indicate that color difference is small；
When △ E is 0.5~1.0, indicate that color difference is small to medium；
When △ E is 1.0~2.0, indicate that color difference is medium；
When △ E is 2.0~4.0, indicate that color difference has gap；
As △ E > 4.0, indicate that color difference is very big.
2. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: a step
According to mass ratio, alkyd resin: ethyl acetate=1:1 in rapid.
3. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: b step
The weight ratio 2.67:40:10 of nano-titanium dioxide to be measured, solvent and bead in rapid.
4. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: b step
It is shaken in rapid using quick worker's oscillator.
5. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: b step
45~60min of concussion mixing in rapid.
6. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: c step
Drying temperature is 40~60 DEG C in rapid.
7. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: c step
Detection uses five angle color difference meter of MA68 in rapid.
8. a kind of method for detecting nano-titanium dioxide down flop property according to claim 1, it is characterised in that: c step
Silk stick spreader scraping blade is used in rapid.
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| CN106018294A (en) | 2016-10-12 |
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